AU1593400A - Method and apparatus for regulating an atmosphere - Google Patents

Abstract

A method and an apparatus for regulating an atmosphere in an essentially closed space are described. The atmosphere contains a condensable substance, inert gas and oxygen, and the method comprises the following steps: withdrawing said atmosphere from the space and passing the same, forming a process gas flow to a concentrator unit wherein said condensable substance is separated from the rest of said process gas flow; returning at least a part of said process gas flow to the space; and bringing said condensable substance from said concentrator unit to a condensation unit and condensing said condensable substance in said condensation unit.

Description

WO 00/29798 1 PCT/SE99/02068 METHOD AND APPARATUS FOR REGULATING AN ATMOSPHERE FIELD OF INVENTION The present invention relates generally to a method and 5 an apparatus for regulating the atmosphere in an essen tially closed space. BACKGROUND It is previously known to inert spaces, into which ob jects are brought and continuously treated. These 10 spaces often contain condensable substances, such as volatile organic compounds (VOC), e.g. solvents, and hydrocarbons. The object of the inerting process is to regulate the atmosphere, e.g. to keep the level of O on a level at which the atmosphere is non-explosive. 15 Another reason to keep the O: low is to maintain the quality of the treated objects because a high 0, level may have a detrimental effect on the final result of the treatment. A preferred inert gas supplied to the space is e.g. 20 nitrogen. In this kind of inertion, a large flow of nitrogen to the inerted space is often needed which leads to large costs for nitrogen. Because there is solvent vapour in the space the outgoing process flow from the space will contain not only nitrogen and oxy 25 gen but also e.g. solvent vapour as well. This means additional costs for the solvent and also for environ mental influence. Also, in many countries stricter en vironmental requirements have required investment in purifying equipment in order to keep the amount of dis 30 charged VOC low and thereby to continue with the opera tion.

WO 00/29798 2 PCT/SE99/02068 The European patent publication EP-0 094 172 discloses a method and an apparatus for recovering solvent vapour from an oven chamber or driver wherein a material bal ance is maintained with respect to the chamber atmos 5 phere. The atmosphere is withdrawn from the oven at a substantially constant flow rate and the uncondensed gas stream is returned to the oven at a rate that de pends on sensed changes in the solvent vapour concen tration. Thereby the combined rates at which solvent 10 vapour is formed in said oven and at which the uncon densed gas stream is returned to the oven mass balance the rate at which the oven atmosphere is withdrawn from the oven. A problem with the described method and apparatus is 15 that that the requirements for low discharges of VOC are not fulfilled in a cost-efficient way. OBJECT OF THE INVENTION An object of the present invention is to provide a method and an apparatus for regulating the atmosphere 20 in an essentially closed space whereby the above men tioned drawbacks of prior art are avoided or at least mitigated and which are cost-efficient and limits the amount of discharged VOC. SUMMARY OF THE INVENTION 25 The invention is based on the realisation, that the outgoing process gas flow can be purified in a cost efficient way by means of a combination of a concentra tor and a condensation plant. According to a first aspect of the invention there is 30 provided a method for regulating an atmosphere in an WO 00/29798 3 PCT/SE99/02068 essentially closed space, said atmosphere containing a condensable substance, inert gas and oxygen, comprising the following steps: a) withdrawing said atmosphere from the space and passing the same, forming a process 5 gas flow to a concentrator unit wherein said condens able substance is separated from the rest of said pro cess gas flow; b) returning at least a part of said process gas flow to the space; and c) bringing said condensable substance from said concentrator unit to a 10 condensation unit and condensing said condensable sub stance in said condensation unit. According to a second aspect of the invention there is provided an apparatus for regulating an atmosphere in an essentially closed space, said atmosphere comprising 15 condensable substance, said apparatus comprising a source of inert gas connected to said space, and a con densation unit for condensation of said condensable substance, characterised in that the apparatus further comprises a concentrator unit provided between said 20 space and said condensation unit, said concentrator unit increasing the level of condensable substance in the flow leaving the concentrator unit to the condensa tion unit compared to that of the flow entering the concentrator unit from the space. 25 Further preferred embodiments are defined in the de pendent claims. BRIEF DESCRIPTION OF DRAWINGS The invention will now be described, by way of example only, with reference to the accompanying drawings, in 30 which: WO 00/29798 4 PCT/SE99/02068 FIG. 1 is a block diagram showing an apparatus accord ing to the invention for maintaining a desired atmos phere in an essentially closed space; FIG. 2 is a diagram showing a concentrator shown in 5 FIG. 1 in more detail; and FIG. 3 is a block diagram of an alternative embodiment of an apparatus according to the invention for main taining a desired atmosphere in an essentially closed space. 10 DETAILED DESCRIPTION OF THE INVENTION In the following, a first embodiment of an apparatus and a process according to the invention for treatment of objects in an essentially closed space will be de scribed with reference to Figs. 1 and 2. The objects 15 (not shown) that are to be treated are moved into and through an essentially closed space 2. The space 2 is well known in the art and comprises openings for the objects to be treated, in some cases some type of gas curtain or other device in order to minimise the amount 20 of oxygen entering the space through the openings etc. The space 2 is connected to a concentrator 5 by means of an outgoing conduit 3 and an ingoing conduit 4. An outlet valve 6 is provided in the ingoing conduit 4, the function of which valve will be described later. 25 The concentrator 5 is in turn connected to a cryo con densation plant (CCP) 9 through an outgoing conduit 7 and an ingoing conduit 8. Finally, there is provided a source of liquid nitrogen (LIN source) 10 connected to the CCP 9 through a con- WO 00/29798 5 PCT/SE99/02068 duit 11. The LIN source 10 is also connected to the space 2 through an evaporator 12 and conduits 13 and 14. The conduit 13 also connects to the CCP 9. The operation of the above-described apparatus will be 5 described in the following. At start-up, the 02 level in the space 2 exceeds a desired level, e.g. 3%. In or der to lower the 0 level pure nitrogen is conducted to the space 2 from the LIN source 10 through the evapora tor 12 and conduits 13 and 14. Thus, the function of 10 the evaporator 12 is to avoid having nitrogen in liquid form enter the space 2, which would lead to damage to the space and objects therein. Nitrogen is supplied from the LIN source 10 to the space 2 until the 0: level therein is lowered to the 15 desired level. The objects to be treated, such as glass bottles or video tapes, are then brought into and through the space 2 through openings (not shown) pro vided therefor. Nitrogen is constantly supplied to the space 2 in order to keep the oxygen level on the de 20 sired level, because new oxygen constantly leaks into the space 2. In order to maintain the pressure in the space 2, a flow of process gas comprising nitrogen, solvent vapour and oxygen will then be conducted by means of a fan (not shown) from the space 2 through the 25 outgoing conduit 3 and into the concentrator 5. The fan can be provided in either conduit 3 or conduit 4. The concentrator 5 will now be described in detail with reference to FIG. 2. The process gas flow enters the concentrator 5 through the conduit 3 and is brought to 30 one of two purifying beds 20a, 20b. There is provided a valve 21a-d in each inlet and outlet of the beds, by WO 00/29798 6 PCT/SE99/02068 which valves the bed to be used for purifying the pro cess gas flow is selected. The bed not used for puri fying the process gas flow is then shut off by means of the valves 21a-d. If e.g. bed 20a is to be used, valves 5 21a and 21b are open whereas valves 21c and 21d are closed. The beds 20a, 20b comprise some suitable purifying material, such as zeolite or active carbon. When the process gas flow is led through the beds, the solvent 10 vapour is separated from the process gas and is re tained in the purifying beds. The purified process gas flow then leaves the concentrator via the conduit 4. The beds 20a, 20b are also connected to the conduits 7 and 8 through valves 22a, 22b and 22c, 22d, respec 15 tively. These connections are used when the beds are to be cleaned, i.e., when they are saturated with solvent. This cleaning process will now be described. The conduits 7 and 8, together with the concentrator 5 and the CCP 9, form an essentially closed system for 20 nitrogen. A fan (not shown) is provided in the conduit 8 for the circulation of the nitrogen. There is also provided a heater 23 in the conduit 8 for heating the nitrogen that is about to enter the concentrator 5, see FIG. 2. The nitrogen entering the concentrator from 25 conduit 8 is brought to the one of the beds 20a, 20b that is saturated with solvent and therefore presently not used for purifying the process gas flow from the space 2. The selection of bed 20a, 20b is effected by means of valves 22a-d. Thus, when bed 20a is used for 30 purifying the process gas flow, the nitrogen from con duit 8 is brought to the saturated bed 20b and vice WO 00/29798 7 PCT/SE99/02068 versa. Thus, when valve 21a is open then valve 22a must be closed and vice versa, i.e., the two valves 21a, 22a must not be open at the same time. However, it is pos sible for the two valves 21a, 22a to be closed at the 5 same time, e.g. when the bed 20a has been cleaned but the other bed 20b is still functioning for purifying the process gas flow. The same applies for the other valve pairs 21b, 22b etc. When the heated nitrogen enters the bed 20a or 20b from 10 conduit 8, the solvent in the bed is evaporated and brought with the heated nitrogen flow leaving the con centrator 5 through the conduit 7 to the CCP 9. In that way the selected bed is cleaned and can thereafter be used to purify the incoming process gas from the space 15 2. The function of the CCP 9 will now be described. It works according to the principles of cryo condensation, which will now be explained. In a cryo condensation plant for condensing e.g. solvent vapour, the effi 20 ciency depends on the concentration of solvent in the process gas. At higher solvent concentrations, a larger part of the cooling effect can be used for condensation of solvent. At lower concentration a larger part of the cooling effect will be used for cooling nitrogen, and 25 this leads to a less efficient use of the cooling ca pacity. In other words, in order to condense the same amount of solvent a much larger amount of LIN would be needed for cooling in the case no concentrator was used. 30 Thus, the incoming nitrogen-solvent flow from conduit 7 is cooled to a very low temperature, whereby a major WO 00/29798 8 PCT/SE99/02068 part of the solvent is condensed. The cooling is effec ted by means of liquid nitrogen brought from the LIN source 10 via the conduit 11. The CCP 9 then works as a heat exchanger, wherein the liquid nitrogen from the 5 LIN source is evaporated thereby cooling the nitrogen solvent flow coming from the concentrator 5. The condensed solvent is collected and can thereafter be returned to the inerted space 2 and reused in the process by means of some suitable piping means, shown 10 as arrow 26 in the figures. Thus, this reuse of solvent provides an inexpensive and effective means for lower ing the costs for solvent. Due to the concentrator 5, the cooling process in the CCP 9 is a very effective one because the nitrogen 15 solvent flow from the concentrator 5 contains a rela tively large portion of solvent. The evaporated pure nitrogen from the LIN source 10, after being used for cooling, is then carried to the space 2 as a part of the nitrogen added through conduit 20 13. In normal operation, when limited amounts of oxygen is leaking into the space 2, the nitrogen used for the cryo condensation and the amount of nitrogen needed for inerting the space 2 is essentially balanced, i.e., all 25 nitrogen used for cooling the CCP goes directly onward to the inerted space 2 and small amounts of or no ni trogen has to be used in the CCP that can not be used in the inerted space 2. This means that there is no additional cost for the cryo condensation process in 30 the CCP 9. In effect, in addition to working as a con- WO 00/29798 9 PCT/SE99/02068 denser, the CCP 9 also functions as an evaporator, fur ther increasing the cost-efficiency of the inventive method and apparatus. A second embodiment of the invention will now be de 5 scribed with reference to FIG. 3. The only change from the embodiment described with reference to Figs. 1 and 2 lies in the CCP 9. In the first embodiment, this functioned as a heat exchanger with two separate sys tems, viz. the system connected to the concentrator 5 10 with the function to condense the solvent and the sys tem connected to the LIN source 10 with the function to cool the nitrogen carrying the solvent, respectively. In this second embodiment, the CCP works in a different way. 15 As seen in FIG. 3, the CCP 9 is still connected to the LIN source 10 and the liquid nitrogen supplied through conduit 11 is used for cooling. However, instead of be ing carried to the space 2, the then evaporated nitro gen used for cooling is supplied to the concentrator 5 20 through the conduit 8. This nitrogen is heated by heater 23, see FIG. 2, before being brought to one of the beds 20a, 20b to be cleaned, just as in the first embodiment. In this second embodiment, however, the fan (not shown) used for circulating the nitrogen in con 25 duit 8 can be omitted, as the pressure from the LIN source 10 is sufficient for forcing the nitrogen through the system. After leaving the concentrator 5, the nitrogen used for cleaning the beds is carried through conduit 7 to the 30 CCP 9, wherein the solvent is condensed. Thereafter, the nitrogen, now with only a minor part of solvent, is WO 00/29798 10 PCT/SE99/02068 lead to the space 2 for inertion. Thus, the system CCP 9, concentrator 5 and conduits 7, 8 no longer forms a closed system for nitrogen. This second embodiment provides several advantages. 5 Firstly, the fan in conduit 8 can be omitted, thus sav ing costs. Secondly, the nitrogen supplied through this conduit 8 is pure, i.e., it contains essentially no oxygen as it comes essentially directly from the LIN source 10. This eliminates the hazards connected to the 10 heater 23 as already small amounts of oxygen in contact therewith can cause an explosion. The self-regulating system of inerting nitrogen coming from the CCP 9 and the evaporator 12 will now be de scribed with reference to FIG. 1. As is seen in that 15 figure, there are provided two pressure controllers 28, 29 in conduit 13 and in the conduit 14 leaving the evaporator 12, respectively. The set pressure value of controller 28 is slightly higher than that of control ler 29, e.g. 200 mbar and 190 mbar, respectively. The 20 nitrogen in conduit 13 then comes primarily from the CCP 9 and only in case there is not sufficient nitrogen supply therefrom, i.e., the pressure drops in conduit 13 before pressure controller 28, nitrogen will be sup plied from the evaporator 12 and conduit 14. In that 25 way it is ensured, that the nitrogen used for cooling the CCP 9 also will be used for inerting the space 2 and that nitrogen coming from the LIN source 10 through the evaporator 12 will be used only in case the nitro gen used for cooling is not sufficient for inerting the 30 space 2. Thus, this provides a very cost-efficient way of reducing the amount of LIN used.

WO 00/29798 11 PCT/SE99/02068 The function of the valve 6 will now be described with reference to FIG. 1. A fundamental feature of the pro cess is that oxygen leaks into the space and an in erting gas, e.g. nitrogen, must therefore be supplied 5 to the space 2. Oxygen and nitrogen together with sol vent vapour is carried as a process gas flow from the space 2 to the concentrator 5. The nitrogen together with oxygen is then returned to the space 2 through conduit 4. In case all the nitrogen-oxygen mixture is 10 returned, this would cause an excess pressure in the space 2. Therefore, some of this nitrogen-oxygen mix ture is bled off through valve 6 and into the surround ing environment. This has been made feasible due to the fact that this nitrogen-oxygen mixture is essentially 15 free of solvent vapour and thus does not constitute an environmental hazard. By using the method and the apparatus according to the invention, the consumption of LIN can be substantially reduced. It has been experimentally shown, that the LIN 20 consumption can be lowered by a factor 8-10. The number of times the nitrogen can be reused depends on how much oxygen is leaking into the space 2. In addition, the condensed solvent can be brought back to the process, whereby the amount of added solvent can be reduced. The 25 LIN used for reducing the level of oxygen can be used not only for that but also to condense the solvent af ter the concentrator. Often when using solely cryogen condensation the re quirements on VOC discharge can not be fulfilled. With 30 the method and the apparatus according to the inven tion, wherein also a concentrator is used, the VOC dis charge can be kept on a low level complying with the WO 00/29798 12 PCT/SE99/02068 requirements also in countries with very strict rules regarding VOC discharge. In view of the foregoing description it will be evident to a person skilled in the art that various modifica 5 tions may be made within the scope of the claims. For example, although two cleaning beds have been shown, any number of beds can be used. If only one bed is used, the process is run intermittently, i.e., the pro cess is run until the bed is saturated with solvent and 10 then the inerting process is shut down and the process cleaning the bed is initiated. Also, the inventive method and apparatus are not lim ited to VOC, such as solvents, but is also applicable to other types of condensable substances, such as 15 hydrocarbons.

Claims (9)

1. A method for regulating an atmosphere in an 5 essentially closed space, said atmosphere containing a condensable substance, inert gas and oxygen, comprising the following steps: a) withdrawing said atmosphere from the space and passing the same, forming a process gas flow to a 10 concentrator unit wherein said condensable sub stance is separated from the rest of said process gas flow; b) returning at least a part of said process gas flow to the space; and 15 c) bringing said condensable substance from said con centrator unit to a condensation unit and condens ing said condensable substance in said condensation unit.

2. A method according to claim 1, c h a r a c 20 t e r i s e d i n that said condensing in step c) com prises cryo condensing.

3. A method according to claim 1 or 2, c h a r a c t e r i s e d i n that step a) comprises bringing the process gas flow to a cleaning bed in said concen 25 trator unit and in that step c) comprises evaporating said condensable substance and bringing said condens able substance from said cleaning bed to said condensa tion unit by means of heated inert gas.

4. A method according to any of claims 1-3, 30 c h a r a c t e r i s e d i n that step c) comprises WO 00/29798 14 PCT/SE99/02068 bringing cool inert gas to the condensation unit for effecting said condensing.

5. A method according to claim 4, c h a r a c t e r i s e d i n the additional step d) of bringing 5 said inert gas used for effecting said condensing to the space for inerting the atmosphere therein.

6. A method according to claim 4, characterised in the additional step d) of bringing said inert gas used for effecting said condensing to the concentrator 10 unit for evaporating said condensable substance and bringing said condensable substance from said cleaning bed to said condensation unit.

7. An apparatus for regulating an atmosphere in an essentially closed space (2), said atmosphere com 15 prising condensable substance, said apparatus compris ing a source of inert gas (10) connected to said space (2), and a condensation unit (9) for condensation of said condensable substance, c h a r a c t e r i s e d i n that the apparatus further 20 comprises a concentrator unit (5) provided between said space (2) and said condensation unit (9), said concentrator unit increasing the level of condensable substance in the flow leaving the concentrator unit to the condensation 25 unit (9) compared to that of the flow entering the con centrator unit from the space (2).

8. An apparatus according to claim 7, c h a r a c t e r i s e d i n that said concentrator unit (5) comprises at least one cleaning bed (20a, 20b) con- WO 00/29798 15 PCT/SE99/02068 nected to said space (2) and said condensation unit (9).

9. An apparatus according to claim 8, c h a r a c t e r i s e d i n that said at least one cleaning 5 bed (20a, 20b) comprises zeolite.